HCID 21186574、化合物 → 2,4-Dimethylresorcinol

HRID 1003622

反応式

HRID 1003622 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:10][C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]([O:18]C(=O)C)[C:12]=1[CH3:22])(=O)C>CCOCC>[OH:10][C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]([OH:18])[C:12]=1[CH3:22]

参加物

4

反応物 2

HCID 21186574HCID 21186574、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 694522,4-Dimethylresorcinol収率 62%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a slurry of lithium aluminum hydride (0.56 g, 14.76 mmol) in ether (35 mL) was added 1,3-diacetoxy-2,4-dimethylbenzene (the compound of Preparation 24, 1.65 g, 7.42 mmol in 40 mL of ether) via syringe. The mixture was stirred overnight; then it was carefully quenched with sodium sulfate decahydrate (excess). The mixture was dried with anhydrous sodium sulfate, filtered, and concentrated to give 0.62 g (62%) of 1,3-dihydroxy-2,4-dimethylbenzene as a waxy light yellow solid which had: NMR δ 6.83 (d, J=8 Hz, 1 H), 6.34 (d, J=8.1 Hz, 1 H), 4.71 (s, 2 H), 2.19 (s, 3 H), 2.17 (s, 3 H). There was also a small amount of an impurity observed in the NMR spectrum but the product was found to be suitable for use without further purification. The product was somewhat air sensitive and was used the same day it was synthesized.

後処理

  1. customthen it was carefully quenched with sodium sulfate decahydrate (excess)
  2. dry with materialThe mixture was dried with anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-6f8864b0b3b045f4b437d0aeb89b552e
出典データセット
uspto-grants-2000_04
特許番号
US06046213

関連ノート

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